Reaktion #92966

ord-3fb3bb36420a4dc8b445fa8ebd9d94c6

Lösungsmittel

Reaktionsbedingungen

Temperatur
50°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.ADDITIONTo a mixture of 129 g
  2. 2
    TemperaturThe resulting mixture was heated in a steam bath at 65° C. overnight
  3. 3
    Extraktionextracted with 300 ml
  4. 4
    ExtraktionThe ether extract
  5. 5
    Waschenwas washed successively with 1N sodium hydroxide, water
  6. 6
    Trocknendried over sodium sulfate
  7. 7
    EinengenThe dried ether solution was concentrated
  8. 8
    workup.DISTILLATIONthe oily residue was distilled under reduced pressure
  9. 9
    Sonstigeyielding 152 g

Vorschrift

To a mixture of 129 g. (1 mole) of 2-chlorophenol, 60 g. of potassium hydroxide, 100 ml. of water and 400 ml. of isopropanol was added 1.3 moles (185.9 g.) of 1,4-dichloro-2-butanol with stirring at 50° C. The resulting mixture was heated in a steam bath at 65° C. overnight and extracted with 300 ml. of isopropyl ether. The ether extract was washed successively with 1N sodium hydroxide, water and dried over sodium sulfate. The dried ether solution was concentrated and the oily residue was distilled under reduced pressure yielding 152 g. of an oily substance (b.p. 130°-131° C./0.01 mm.).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04609735uspto-grants-1986_09